Reacción #8919

ord-a7fe96d87c28497989d234d770dec179

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otropartitioned between EtOAc and saturated aqueous NaHCO3 solution
  2. 2
    OtroThe organic layer was separated
  3. 3
    Lavadowashed with aq. NaHCO3, brine
  4. 4
    Secadodried (Na2SO4)
  5. 5
    Filtraciónfiltered
  6. 6
    Otroevaporated
  7. 7
    OtroThe residue was purified on a silica gel flash chromatography column
  8. 8
    Lavadoeluted with 0–75% EtOAc-hexane
  9. 9
    OtroEvaporation of the purified fractions
  10. 10
    Otrodrying in vacuo

Procedimiento

To a solution of the product of Step A in 4 mL DMF was added 0.125 g (0.698 mmol) of 1-bromopinacolone and 0.455 g (1.39 mmol) of Cs2CO3. The reaction mixture was stirred at room temperature for 1 h, then partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was separated, washed with aq. NaHCO3, brine, dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–75% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07091216B2uspto-grants-2006_08